ESU-050

Lecture - Flavor Emulsion/Encapsulation

Topics to be covered today
1. Flavor Emulsion
Morphology of Microcapsules:
Depends mainly on –
the core material and the deposition process of the shell.

1- MONONUCLEAR (core-shell) microcapsules contain the shell around

the core.

2- POLYNUCLEAR capsules have many cores enclosed within the shell.

3- MATRIX encapsulation in which the core material is distributed

homogeneously into the shell material.

- In addition to these three basic morphologies, microcapsules can

also be mononuclear with multiple shells, or they may form clusters of
microcapsules.
 How to make the encapsulation of
flavors?

 Preparation of emulsion
Process to encapsulate flavors
Spray drying
Single Emulsion

Multiple Emulsion
 0.2 – 50 mm Macroemulsions
 0.01 – 0.2 mm Microemulsions
 50 – 1000 nm Nanoemulsions
 Oil in water emulsion (o/w) Water in oil emulsion (w/o)
 Water is the dispersion medium  Oil is the dispersion medium and
and oil is the dispersed phase. water is the dispersed phase.
 Water soluble drugs are more  Oil soluble drugs are more quickly
quickly released from o/w released from w/o emulsions .
emulsions.  They are preferred for
 They are preferred for formulations meant for external
formulations meant for internal use like creams.
 They are greasy and not water
use as bitter taste of oils can be washable.
masked.
 They are used externally to
 They are non greasy and easily prevent evaporation of moisture
removable from the skin surface. from the surface of skin e.g. Cold
 They are used externally to cream.
provide cooling effect e.g.  W/O emulsions go not give a
vanishing cream positive conductivity test as oil is
 O/W emulsions give a positive the external phase which is a poor
conductivity test as water is the conductor of electricity.
external phase which is a good
conductor of electricity.
Application of Emulsion
➢ Oral, rectal and topical administration of oils and oil-soluble
Foods/drugs.
➢ -The unpleasant taste or odor can be masked by
emulsification.
➢ - The absorption and penetration of medicament are enhanced
by emulsification.
➢ - Intramuscular injections of water-soluble drugs or vaccine to
provide slow release.
➢ - The use of sterile stable i.v emulsion containing fats,
carbohydrates and vitamins as a potential nutrition.
 Selection of Emulsifying agents (emulsifiers):
➢ An emulsifying agent is any material that enhances the stability of
an emulsion (i.e. Prevention of coalescence and reducing creaming).
➢ The ideal emulsifying agent is colourless, odourless, tasteless, non-
toxic, non-irritant and able to produce stable emulsions at low
concentrations.
➢ Examples of Emulsifying agent
1. Carbohydrate Materials:
- Acacia, Tragacanth, Agar, Pectin. o/w emulsion.
2. Protein Substances:
- Gelatin, Egg yolk, Caesin o/w emulsion.
3. High Molecular Weight Alcohols:
-Stearyl Alcohol, Cetyl Alcohol, Glyceryl Mono stearate o/w emulsion,
cholesterol w/o emulsion.
 -Anionic, Cationic, Nonionic
-o/w emulsion
-w/o emulsion
5. Finely divided solids
- Bentonite, Magnesium Hydroxide, Aluminum Hydroxide o/w emulsion.
Test for identification of emulsion type
➢ Dilution test (miscibility test)
➢ Staining test (dye solubility test)
➢ Conductivity measurement
➢ Fluorescence test
➢ Film theory or adsorption theory
➢ Viscosity theory
➢ Wedge theory
➢ Interfacial tension theory
Film theory or adsorption theory
➢ As per this theory, the added emulsifying agent forms a
mechanical film by getting adsorption at the interface of the
liquid and offers stability to the emulsion. However, this
theory could not explain the formation of type of emulsion.
Viscosity theory
➢ As per this theory, an increase in viscosity of an emulsion
will lead to an increase in stability. This theory failed to
explain about the milk which shows considerable stability
even though its viscosity is less.
➢ According to this theory, monovalent soap like sodium
stearate give o/w type emulsion and divalent soap like calcium
stearate give w/o type emulsion. This was explained by
successful accommodation of the soap molecules to give the
type of emulsion.
Interfacial tension theory
➢ In accordance with this theory the added emulsifying agent
reduces the interfacial tension between the oil and water
phases and thus a stable emulsion is formed. This theory could
not explain the formation of type of emulsion.
➢ An ideal emulsifying agent should posses the following
characteristics:
➢ It should be able to reduce the interfacial tension between the two
immiscible liquids.
➢ It should be physically and chemically stable , inert and
compatible with the other ingredients of the formulation.
➢ It should be non irritant and non toxic in the conc., used.
➢ It should be organoleptically inert i.e. should not impart any color
, odour or taste to the preparation.
➢ It should be able to produce and maintain the required viscosity of
the preparation.
➢ It should be able to form a coherent film around the globules of
the dispersed phase and should prevent the coalescence of the
droplet of the dispersed phase.
➢ Depending on the use, emulsions should be packed in suitable
containers. Emulsions meant for oral use are usually packed in
well filled bottles having an air tight closure.
➢ Light sensitive products are packed in amber colored bottles.
➢ For viscous emulsions, wide mouth bottles should be used. The
label on the emulsion should mention that these products have
to be shaken thoroughly before use.
➢ External use products should clearly mention on their label that
they are meant for external use only.
➢ Emulsions should be stored in a cool place but refrigeration
should be avoided as this low temperature can adversely effect
the stability of preparation.
➢ Microbial contamination may occur due to:
➢ contamination during development or production of emulsion or
during its use.

➢ Usage of impure raw materials

➢ Poor sanitation conditions
➢ Invasion by an opportunistic microorganisms.
➢ Contamination by the consumer during use of the product..
➢ Precautions to prevent microbial growth ;
➢ Use of uncontaminated raw materials
➢ Careful cleaning of equipment with steam .
The methods commonly used to prepare emulsions can be
divided into two categories
A) Trituration Method
This method consists of dry gum method and wet gum method.

➢ Dry Gum Method

In this method the oil is first triturated with gum with a little
amount of water to form the primary emulsion. The trituration is
continued till a characteristic ‘clicking’ sound is heard and a
thick white cream is formed. Once the primary emulsion is
formed, the remaining quantity of water is slowly added to form
the final emulsion.
"4:2:1" formula
4 parts (volumes) of oil
2 parts of water
1 part of gum

➢ Wet Gum Method

As the name implies, in this method first gum and water are
triturated together to form a mucilage. The required quantity of
oil is then added gradually in small proportions with thorough
trituration to form the primary emulsion.
Once the primary emulsion has been formed remaining quantity
of water is added to make the final emulsion.
"4:2:1" formula
4 parts (volumes) of oil
2 parts of water
1 part of gum

Mortar and Pestle Homogeniser

➢ This method is employed for preparing emulsions containing
volatile and other non-viscous oils. Both dry gum and wet gum
methods can be employed for the preparation.
➢ As volatile oils have a low viscosity as compared to fixed oils,
they require comparatively large quantity of gum for
emulsification.
➢ In this method, oil or water is first shaken thoroughly and
vigorously with the calculated amount of gum. Once this has
emulsified completely, the second liquid (either oil or water) is
then added all at once and the bottle is again shaken vigorously
to form the primary emulsion. More of water is added in small
portions with constant agitation after each addition to produce
the final volume.
➢ Mechanical stirrers
➢ Propeller type mixers
-Turbine mixers
- Homogenizers
➢ Colloid mills
➢ Ultrasonifiers

Mechanical stirrers Colloidal mill

➢ An emulsion is said to be stable if it remains as such after its
preparation , that is the dispersed globules are uniformly
distributed through out the dispersion medium during its
storage. The emulsion should be chemically stable and there
should not be any bacterial growth during it shelf life.
➢ Emulsion instability may either reversible or irreversible and
manifest in the following ways:-
1) Cracking (irreversible instability)
2) Flocculation
3) Creaming
4) Phase inversion
 Cracking means the separation of two layers of disperse and
continuous phase , due to the coalescence of disperse phase
globules which are difficult to redisperse by shaking.
 Cracking may occurs due to following reasons:-

i. By addition of emulsifying agent of opposite type

ii. By decomposition or precipitation of emulsifying agent
iii. By addition of common solvent
iv. By microorganisms
v. Change in temperature
vi. By creaming
 In flocculated state the secondary interaction (van der waals
forces) maintain the droplets at a defined distance of
separation.

 Application of shearing stress to the formulation (shaking) will

redisperse these droplets to form a homogeneous formulation.

 Although flocculation may stabilise the formulation, there is

also possibility that the close location of droplets would enable
droplet coalescence to occur if the mechanical properties of
the interfacial film are compromised.
 Creaming may be defined as the upward movement of
dispersed globules to form a thick layer at the surface of
emulsion.
 Creaming is temporary phase because it can be re-distributed
by mild shaking or stirring to get again a homogenous
emulsion.
a. Radius of globules
b. Difference in density of disperse phase and continuous phase
c. Viscosity of dispersion medium
d. Storage condition

4) Phase inversion:-
➢ Phase inversion means the change of one type of emulsion
into other type, that is oil in water emulsion changes into
water in oil type and vice-versa.
i. By the addition of an electrolyte

ii. By changing the phase-volume ratio

iii. By temperature change

iv. By changing the emulsifying agent

 The phase inversion can be minimised by keeping concentration of

disperse phase between 30 to 60 % , storing the emulsion in
cool place and using a proper emulsifying agent in adequate
concentration.
 Stability of the active ingredient
 Stability of the excipients
 Visual appearance
 Color
 Odor (development of pungent odor/loss of fragrance)
 Viscosity, extrudability
 Loss of water and other volatile vehicle components
 Concentration of emulsifier
 Particle size distribution of dispersed phases
 pH
 Temperature of emulsification
 Method and rate of cooling
 Texture, feel upon application (stiffness, grittiness, greasiness, tackiness)
 Microbial contamination/sterility
 Release/bioavailability (percutaneous absorption)
 Phase distribution, Phase Inversion (homogeneity/phase separation, bleeding)
Prafull Chavan
School of Bioengineering and Food
Technology
Shoolini University
Village Bajhol, Solan (H.P)
+91 8329700343.(Mob No.)
prafull@shooliniuniversity.com